CN106479313A - A kind of Graphene anticorrosive paint - Google Patents
A kind of Graphene anticorrosive paint Download PDFInfo
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- CN106479313A CN106479313A CN201610878263.1A CN201610878263A CN106479313A CN 106479313 A CN106479313 A CN 106479313A CN 201610878263 A CN201610878263 A CN 201610878263A CN 106479313 A CN106479313 A CN 106479313A
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D163/00—Coating compositions based on epoxy resins; Coating compositions based on derivatives of epoxy resins
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
- C09D5/08—Anti-corrosive paints
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/40—Additives
- C09D7/60—Additives non-macromolecular
- C09D7/61—Additives non-macromolecular inorganic
- C09D7/62—Additives non-macromolecular inorganic modified by treatment with other compounds
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured additives
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/08—Stabilised against heat, light or radiation or oxydation
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
- C08L2205/035—Polymer mixtures characterised by other features containing three or more polymers in a blend containing four or more polymers in a blend
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Abstract
The invention discloses a kind of Graphene anticorrosive paint, count by weight, be made up of following composition：76 87 parts of model DER671 Tao Shi solid epoxies；22 25 part of 582 type melamine resin；Oronain hectorite draws in 27 28 parts of departments；67 parts of hydroxy boric acid frequency any esters；The Graphene precursor of 0.5 0.7 parts of oxidation modifications；13 parts of γ aminopropyltriethoxywerene werene；57 parts of Nano titanium dioxides；35 parts of Y 311SN type blocked isocyanate curing agents；12 15 parts of calcined kaolins；23 parts of zinc chromates；32 35 parts of solvents；0.2 0.4 parts of paraformaldehydes.The present invention makes the stability of Graphene increase by graphite is carried out with secondary oxidation modification, is conducive to the maximum decay resistance playing Graphene itself, makes the coating prepared have excellent adhesive force, hardness and wearability and resistance to Neutral Salt Spray Corrosion.
Description
Technical field
The invention belongs to technical field of metal anti-corrosion is and in particular to a kind of Graphene anticorrosive paint and preparation method thereof.
Background technology
Use more anticorrosive paint such as organic zinc-rich paint, its conventional epoxy resin, chlorinated rubber, vinyl tree at present
Fat and polyurethane resin are film forming binder.The most commonly used is epoxy zinc-enriched paint, wherein polyamide cure epoxy zinc rich primer
It is the kind applying maximum in organic zinc-rich primer.The rustless property of organic type coating is more slightly worse than inorganic type, electric conductivity, heat-resisting
Property, solvent resistance be not so good as inorganic type.
Six side's honeycomb two-dimension nano materials that Graphene (Graphene) is made up of monolayer carbon atom, it special two
Dimension structure makes it have excellent physical and chemical performance, has caused the research boom of a new round, and may cause in a lot of fields
Revolutionary change.However, Graphene is neither hydrophilic nor oleophylic, seriously hinder its dispersion in any solvent, limit
Application in polymer nanocomposites；In addition chemical reaction is inert etc. hinders its development further.
Graphene oxide (Graphene oxide, GO) is to be prepared by classical Hummers deep oxidation method
Arrive.GO contains on surface substantial amounts of hydroxyl, epoxy radicals, carboxyl isoreactivity oxy radical (according to Lerf-Klinowski model),
And chemical reaction can be carried out with other molecules further, function graphite is prepared by covalent and non-covalent synthetic technology magnanimity
Alkene.
But the oxy radical of surface of graphene oxide makes its heat stability low, is heated and easily degrades, weightless temperature is interval
Narrow, and there is the defect that can only be scattered in intensive polar solvent.So directly prepare anti-corrosion painting by the Graphene of oxidation modification
Material has certain technical difficulty.
Content of the invention
It is an object of the invention to provide a kind of Graphene of oxidation modification is preparing anticorrosive paint, instant invention overcomes oxidation
The oxy radical of graphenic surface makes its heat stability low, the shortcoming of easily degraded of being heated, the Graphene after oxidation modification
The anticorrosive paint prepared has the acid and alkali-resistance antiseptic property more excellent than common anticorrosive paint, higher adhesive force and hard
Degree.
According to an aspect of the present invention, the invention provides a kind of Graphene anticorrosive paint, described Graphene is oxidation
Modified Graphene precursor, counts, Graphene anticorrosive paint is made up of following composition by weight：
76-87 part model DER671 Tao Shi solid epoxy；22-25 part 582 type melamine resin；27-
Oronain hectorite draws in 28 parts of departments；6-7 part hydroxy boric acid frequency any ester；The Graphene precursor of 0.5-0.7 part oxidation modification；1-3
Part γ aminopropyltriethoxy silane；5-7 part Nano titanium dioxide；3-5 part Y-311SN type blocked isocyanate solidifies
Agent；12-15 part calcined kaolin；2-3 part zinc chromate；32-35 part solvent；0.2-0.4 part paraformaldehyde；
The Graphene precursor of described oxidation modification is by following preparation method gained：
1) in reactor, interior temperature control, at -10 DEG C, adds the 6N concentrated sulphuric acid of 20L, opens stirring；
2) add 5kg granularity be the crystalline flake graphite of 400 mesh to reactor, make crystalline flake graphite all be immersed in concentrated sulphuric acid
In, stir 60min at -10 DEG C；
3) reactor is warming up to 5 DEG C of stirring 20min；
4) the cooling circulation of stopped reaction kettle, instills the sodium nitrate adding 2N, exothermic heat of reaction in reactor；By Deca
Speed controlling temperature in reactor to be 5-10 DEG C, 10 DEG C of reaction 2h after completion of dropping；
5) to the potassium permanganate solution 6L of Deca 3N in reactor, peristaltic pump is taken to control rate of addition, point three phases
Control different rate of addition；First stage rate of addition controls in 80ml/min, and dripping quantity is 2L；Second stage Deca speed
Degree controls in 10ml/min, and dripping quantity is 3L；Three phases rate of addition controls in 60ml/min, and dripping quantity is 1L；Deca
Finish rear reactor and be warming up to 40 DEG C of reaction 2h；
6) backflow, back flow reaction 3h are warming up to by 40 DEG C with the heating rate of 20 DEG C/h
7) backflow is cooled to 35 DEG C with the rate of temperature fall of 40 DEG C/h after finishing, then in reactor Deca 10wt% double
Oxygen water 4kg；It is cooled to room temperature after completion of dropping, take anti-riot centrifuge with standing point after centrifugation 10min under the rotating speed of 100rpm
Layer；
8) lower floor's material is separated and be placed in high speed dispersing shear machine, in cutter, then add 3kg PEG800
Dispersing shear 30min under the rotating speed of 1400rpm, adds the sodium hypochlorite of 2L10wt% to be aoxidized, under the rotating speed of 1400rpm
Dispersing shear 30min obtains the Graphene precursor of gluey oxidation modification, in the present invention in the presence of PEG800 to oxidation after
Graphite carries out secondary oxidation, not only increases graphene thermal stability, and heat stability increases.
Described solvent is by weight by dimethylbenzene：Isopropyl acetate：Glycol dimethyl ether：Acetone=13：27：20：21
Composition.
Preferably, count by weight, Graphene anticorrosive paint is made up of following composition：
80 parts of model DER671 Tao Shi solid epoxies；23 part of 582 type melamine resin；Chlorine draws in 27 parts of departments
Ammonium hectorite；7 parts of hydroxy boric acid frequency any esters；The Graphene precursor of 0.6 part of oxidation modification；2 parts of gamma-amino propyl group three ethoxies
Base silane；6 parts of Nano titanium dioxides；4 parts of Y-311SN type blocked isocyanate curing agents；13 parts of calcined kaolins；3 parts of chromium
Sour zinc；34 parts of solvents；0.3 part of paraformaldehyde.
According to another aspect of the present invention, the invention provides a kind of preparation method of Graphene anticorrosive paint, including
Following steps：
1) solvent is inserted in ultrasonic reactor, add the Graphene precursor of oxidation modification, be warming up to 60 DEG C of stirrings ultrasonic
Dispersion 20min；
2) it is cooled to 40 DEG C and add paraformaldehyde, zinc chromate, γ aminopropyltriethoxy silane stirring 30min successively；
3) ball mill is taken to draw oronain water to DER671 Tao Shi solid epoxy, 582 type melamine resins, department
Pyroxene, calcined kaolin obtain resin combination after being ground being less than 20 microns to D90, then add in resin combination and receive
Meter level titanium dioxide obtains titania-doped resin combination；
4) titania-doped resin combination is added step 2) in system in, dispersed with stirring 1h, then add again
Plus obtain Graphene after grinding 150min after hydroxy boric acid frequency any ester and Y-311SN type blocked isocyanate curing agent stirring 4h
Anticorrosive paint.
Compared with prior art, the Graphene anticorrosive paint of present invention preparation has advantages below：
1st, the present invention makes the stability of Graphene increase by graphite is carried out with secondary oxidation modification, is conducive to maximum performance
The decay resistance of Graphene itself, make the coating prepared have excellent anticorrosive property, high temperature resistant, weatherability, alkali resistance,
The advantages of impact resistance and artificial ageing resistance；
2nd, the Graphene precursor agglutination of the oxidation modification of present invention preparation, was mixed with the other components in coating beneficial to the later stage
Close, make product quality more stable and uniform.
Specific embodiment
For making the object, technical solutions and advantages of the present invention of greater clarity, with reference to specific embodiment, to this
Invention further describes.It should be understood that these descriptions are simply exemplary, and it is not intended to limit the scope of the present invention.
Embodiment 1
The Graphene precursor of preparation oxidation modification：
1) in reactor, interior temperature control, at -10 DEG C, adds the 6N concentrated sulphuric acid of 20L, opens stirring；
2) add 5kg granularity be the crystalline flake graphite of 400 mesh to reactor, make crystalline flake graphite all be immersed in concentrated sulphuric acid
In, stir 60min at -10 DEG C；
3) reactor is warming up to 5 DEG C of stirring 20min；
4) the cooling circulation of stopped reaction kettle, instills the sodium nitrate adding 2N, exothermic heat of reaction in reactor；By Deca
Speed controlling temperature in reactor to be 5-10 DEG C, 10 DEG C of reaction 2h after completion of dropping；
5) to the potassium permanganate solution 6L of Deca 3N in reactor, peristaltic pump is taken to control rate of addition, point three phases
Control different rate of addition；First stage rate of addition controls in 80ml/min, and dripping quantity is 2L；Second stage Deca speed
Degree controls in 10ml/min, and dripping quantity is 3L；Three phases rate of addition controls in 60ml/min, and dripping quantity is 1L；Deca
Finish rear reactor and be warming up to 40 DEG C of reaction 2h；
6) backflow, back flow reaction 3h are warming up to by 40 DEG C with the heating rate of 20 DEG C/h
7) backflow is cooled to 35 DEG C with the rate of temperature fall of 40 DEG C/h after finishing, then in reactor Deca 10wt% double
Oxygen water 4kg；It is cooled to room temperature after completion of dropping, take anti-riot centrifuge with standing point after centrifugation 10min under the rotating speed of 100rpm
Layer；
8) lower floor's material is separated and be placed in high speed dispersing shear machine, in cutter, then add 3kg PEG800
Dispersing shear 30min under the rotating speed of 1400rpm, adds the sodium hypochlorite of 2L10wt% to be aoxidized, under the rotating speed of 1400rpm
Dispersing shear 30min obtains the Graphene precursor of gluey oxidation modification.
Dispensing and its preparation：
First, dispensing：Weigh 76 parts of model DER671 Tao Shi solid epoxies by weight；22 part of 582 type tripolycyanamide
Formaldehyde resin；Oronain hectorite draws in 27 parts of departments；6 parts of hydroxy boric acid frequency any esters；The Graphene precursor of 0.5 part of oxidation modification；1
Part γ aminopropyltriethoxy silane；5 parts of Nano titanium dioxides；3 parts of Y-311SN type blocked isocyanate curing agents；12
Part calcined kaolin；2 parts of zinc chromates；32 parts of solvents；0.2 part of paraformaldehyde；
2nd, preparation method
1) solvent is inserted in ultrasonic reactor, add the Graphene precursor of oxidation modification, be warming up to 60 DEG C of stirrings ultrasonic
Dispersion 20min；
2) it is cooled to 40 DEG C and add paraformaldehyde, zinc chromate, γ aminopropyltriethoxy silane stirring 30min successively；
3) ball mill is taken to draw oronain water to DER671 Tao Shi solid epoxy, 582 type melamine resins, department
Pyroxene, calcined kaolin obtain resin combination after being ground being less than 20 microns to D90, then add in resin combination and receive
Meter level titanium dioxide obtains titania-doped resin combination；
4) titania-doped resin combination is added step 2) in system in, dispersed with stirring 1h, then add again
Plus obtain Graphene after grinding 150min after hydroxy boric acid frequency any ester and Y-311SN type blocked isocyanate curing agent stirring 4h
Anticorrosive paint.
Embodiment 2
Weight proportion：80 parts of model DER671 Tao Shi solid epoxies；23 part of 582 type melamine resin；
Oronain hectorite draws in 27 parts of departments；7 parts of hydroxy boric acid frequency any esters；The Graphene precursor of 0.6 part of oxidation modification；2 parts of gamma-aminos
Propyl-triethoxysilicane；6 parts of Nano titanium dioxides；4 parts of Y-311SN type blocked isocyanate curing agents；13 parts of calcinings are high
Ridge soil；3 parts of zinc chromates；34 parts of solvents；0.3 part of paraformaldehyde.
In the preparation method of preparation and anticorrosive paint and embodiment 1 before the Graphene of oxidation modification in embodiment 2
Preparation method is identical.
Embodiment 3
Weight proportion：Weigh 87 parts of model DER671 Tao Shi solid epoxies by weight；25 part of 582 type tripolycyanamide
Formaldehyde resin；Oronain hectorite draws in 28 parts of departments；7 parts of hydroxy boric acid frequency any esters；The Graphene precursor of 0.7 part of oxidation modification；3
Part γ aminopropyltriethoxy silane；7 parts of Nano titanium dioxides；5 parts of Y-311SN type blocked isocyanate curing agents；15
Part calcined kaolin；3 parts of zinc chromates；35 parts of solvents；0.4 part of paraformaldehyde.
In the preparation method of preparation and anticorrosive paint and embodiment 1 before the Graphene of oxidation modification in embodiment 3
Preparation method is identical.
Metal material surface is applied directly to the anticorrosive paint of embodiment 1-3 preparation, carries out adhesive force, wearability, hard
Degree aspect performance detection, comparative example 1 is the F-C paint anticorrosive paint of commercially available Shandong China；Formula used by comparative example 2 and preparation method with
Embodiment 1 is identical, and unique difference is the Graphene precursor wherein not adding oxidation modification.Result such as table 1：
Table 1 test result
The salt fog of resistance to standard Neutral performance test：Neutral salt spray test is done using standard Neutral salt fog machine.By sample (coating
Amount：240mg/dm2) put into and in salt fog machine, use saline (concentration is 5 weight %, and pH value is 6.5-7.2) to spray at 35 DEG C, observe
Sample changed condition.
Result above shows that the coating of present invention preparation has excellent adhesive force, hardness and wearability and resistance to neutral salt
Mist corrosivity.
Although embodiments of the present invention are described in detail it should be understood that, without departing from the present invention's
In the case of spirit and scope, embodiments of the present invention can be made with various changes, replacement and change.
Claims (3)
1. a kind of Graphene anticorrosive paint, described Graphene is the Graphene precursor of oxidation modification, counts by weight, Graphene
Anticorrosive paint is made up of following composition：
76-87 part model DER671 Tao Shi solid epoxy；22-25 part 582 type melamine resin；27-28 part
Oronain hectorite draws in department；6-7 part hydroxy boric acid frequency any ester；The Graphene precursor of 0.5-0.7 part oxidation modification；1-3 part γ-
Aminopropyltriethoxywerene werene；5-7 part Nano titanium dioxide；3-5 part Y-311SN type blocked isocyanate curing agent；12-
15 parts of calcined kaolins；2-3 part zinc chromate；32-35 part solvent；0.2-0.4 part paraformaldehyde；
The Graphene precursor of described oxidation modification is by following preparation method gained：
1) in reactor, interior temperature control, at -10 DEG C, adds the 6N concentrated sulphuric acid of 20L, opens stirring；
2) add 5kg granularity be the crystalline flake graphite of 400 mesh to reactor, make crystalline flake graphite all dipping in concentrated sulfuric acid, -10
60min is stirred at DEG C；
3) reactor is warming up to 5 DEG C of stirring 20min；
4) the cooling circulation of stopped reaction kettle, instills the sodium nitrate adding 2N, exothermic heat of reaction in reactor；By rate of addition
The temperature in reactor is controlled to be 5-10 DEG C, 10 DEG C of reaction 2h after completion of dropping；
5) to the potassium permanganate solution 6L of Deca 3N in reactor, peristaltic pump is taken to control rate of addition, point three phases control
Different rate of addition；First stage rate of addition controls in 80ml/min, and dripping quantity is 2L；Second stage rate of addition control
In 10ml/min, dripping quantity is 3L to system；Three phases rate of addition controls in 60ml/min, and dripping quantity is 1L；Completion of dropping
Reactor is warming up to 40 DEG C of reaction 2h afterwards；
6) backflow, back flow reaction 3h are warming up to by 40 DEG C with the heating rate of 20 DEG C/h；
7) backflow is cooled to 35 DEG C with the rate of temperature fall of 40 DEG C/h, then to the hydrogen peroxide of Deca 10wt% in reactor after finishing
4kg；It is cooled to room temperature after completion of dropping, take anti-riot centrifuge with stratification after centrifugation 10min under the rotating speed of 100rpm；
8) lower floor's material is separated and is placed in high speed dispersing shear machine, then in cutter add 3kg PEG800 in
Dispersing shear 30min under the rotating speed of 1400rpm, adds the sodium hypochlorite of 2L10wt% to be aoxidized, lower point of the rotating speed of 1400rpm
Dissipate the Graphene precursor that shearing 30min obtains gluey oxidation modification；
Described solvent is by weight by dimethylbenzene：Isopropyl acetate：Glycol dimethyl ether：Acetone=13：27：20：21 compositions.
2. a kind of Graphene anticorrosive paint according to claim 1, described Graphene is the Graphene precursor of oxidation modification, its
It is characterised by：Count by weight, Graphene anticorrosive paint is made up of following composition：80 parts of model DER671 Tao Shi solid rings
Oxygen tree fat；23 part of 582 type melamine resin；Oronain hectorite draws in 27 parts of departments；7 parts of hydroxy boric acid frequency any esters；0.6
The Graphene precursor of part oxidation modification；2 parts of γ aminopropyltriethoxy silanes；6 parts of Nano titanium dioxides；4 parts of Y-
311SN type blocked isocyanate curing agent；13 parts of calcined kaolins；3 parts of zinc chromates；34 parts of solvents；0.3 part of paraformaldehyde.
3. a kind of preparation method of Graphene anticorrosive paint described in claim 1 or 2, comprises the following steps：
1) solvent is inserted in ultrasonic reactor, add the Graphene precursor of oxidation modification, be warming up to 60 DEG C of stirring ultrasonic disperse
20min；
2) it is cooled to 40 DEG C and add paraformaldehyde, zinc chromate, γ aminopropyltriethoxy silane stirring 30min successively；
3) ball mill is taken to draw oronain water brightness to DER671 Tao Shi solid epoxy, 582 type melamine resins, department
Stone, calcined kaolin obtain resin combination after being ground being less than 20 microns to D90, then add nanometer in resin combination
Grade titanium dioxide obtains titania-doped resin combination；
4) titania-doped resin combination is added step 2) in system in, dispersed with stirring 1h, then add hydroxyl again
Graphene is obtained anti-corrosion after grinding 150min after base propylene boric acid frequency any ester and Y-311SN type blocked isocyanate curing agent stirring 4h
Coating.
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| CN107502018A (en) * | 2017-09-22 | 2017-12-22 | 安徽慕曼德家具有限公司 | A kind of scratch resistant environmental protection paint |
| CN107793901A (en) * | 2017-10-20 | 2018-03-13 | 安徽快来防水防腐有限公司 | A kind of production method for the poly-aspartate polyurea water-proof corrosion-inhibiting coating that graphene is modified |
| CN109233562A (en) * | 2018-08-09 | 2019-01-18 | 苏州市泽镁新材料科技有限公司 | A kind of anticorrosive coating for metal surface |
| CN109266220A (en) * | 2018-08-17 | 2019-01-25 | 深圳市福来过科技有限公司 | A kind of anticorrosive paint and its preparation process modified based on graphene |
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| CN109836919A (en) * | 2017-09-29 | 2019-06-04 | 天津工业大学 | A kind of functional graphene oxide corrosion-inhibiting coating and its preparation process |
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| CN112210278A (en) * | 2019-07-12 | 2021-01-12 | 常州市大使涂料有限公司 | Polyurea spraying elastomer for pipeline corrosion prevention |
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| EP3889224A4 (en) * | 2018-11-29 | 2022-08-31 | Toray Industries, Inc. | Graphene anti-corrosion coating |
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